CN104596892A - Gas-solid surface reaction device and measuring method adopting same - Google Patents
Gas-solid surface reaction device and measuring method adopting same Download PDFInfo
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- CN104596892A CN104596892A CN201510070189.6A CN201510070189A CN104596892A CN 104596892 A CN104596892 A CN 104596892A CN 201510070189 A CN201510070189 A CN 201510070189A CN 104596892 A CN104596892 A CN 104596892A
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Abstract
The invention discloses a gas-solid surface reaction device and a measuring method adopting the same, aiming to solve the problem that presently a sample treated under a low-vacuum or positive-pressure condition needs to be exposed to the atmosphere before being transferred to other ultrahigh vacuum environments for follow-up analysis. According to a conventional method, the sample is subjected to low-pressure or high-pressure reaction treatment in a specific reaction vessel, then the reaction vessel is opened, and the sample is taken out and transferred to other ultrahigh vacuum analysis spectrometers; and the problem of secondary contamination of the surface of the sample caused by the atmosphere is obviously hard to avoid in the process. According to the gas-solid surface reaction device provided by the invention, a gas-solid high-pressure reaction can be performed and ultrahigh vacuum can be obtained; and in a high-pressure inflation and reaction process, on-line collection and recordation of temperature and pressure can be realized, and after reaction is finished, a cavity can stay in an ultrahigh vacuum state and the sample can be transferred in vacuum to other connected analysis equipment. Through the gas-solid surface reaction device, secondary contamination on the surface of the sample caused by the atmosphere is completely solved, and meanwhile the working efficiency is effectively improved. The gas-solid surface reaction device is reasonable in design, has a skillful concept and is of great significance on studying of gas-solid surface reaction.
Description
Technical field
The present invention relates to a kind of Gas-solid surface reaction unit and adopt it to carry out method for measuring, especially not only can provide ultrahigh vacuum but also the Gas-solid surface reaction chamber of reaction under high pressure can have been carried out, mesohigh reaction chamber of the present invention be positioned at ultrahigh vacuum cavity and itself and share a set of specimen holder with ultrahigh vacuum cavity.The present invention can be used in the compatibility of material in specific reaction atmosphere and surface reaction research, has important use value.
Background technology
In several atomic layers near solid surface, atom has many physicochemical characteristicss differing from solid interior.Therefore, the arranging situation of atom in the several atomic layer in material surface scientific research surface, electronic state, be adsorbed on foreign atom on surface or molecule, and the electronic state of foreign impurity in the several atomic layer in surface and other physico-chemical property.In order to improve the conformability of material to environment, need to further investigate material surface Surface Physical Chemistry of (temperature, pressure) under environment for use condition and change, correlative study achievement can be material surface modifying technology and new material research and development provide technical support.
Modern surface science analytical technology, as technology such as XPS, AES, SIMS and STM, when carrying out the surface analysis of material, needs be better than 10 usually
-6carry out in the ultra-high vacuum environment of more than Pa.Ultra-high vacuum environment tool has the following advantages: in (1) sample surfaces short time, can not be subject to Residual Gas and pollute; (2) electronics can be reduced to be absorbed or scattering probability by residual gas molecule; (3) for some vacuum component provides stable working environment.But in some engineering-environment, reaction atmosphere is low vacuum even positive pressure, in order to original position carries out these surface reactions research, new gas-solid reaction device must be designed.
After sample processes under low vacuum or positive pressure, usually need to transfer to other ultra-high vacuum environment and carry out subsequent analysis.Conventional method needs first complete paired samples low pressure or reaction under high pressure process in specific reaction vessel, then opens reaction vessel and takes out sample and transfer to other ultrahigh vacuum analysis environments.But the method to be difficult to avoid turning in sample process air to the secondary pollution of material surface, and then affects experimental result.
Summary of the invention
Goal of the invention of the present invention is: need to expose air after processing under low vacuum or positive pressure for current sample and just can be transferred to the problem that other ultra-high vacuum environment carries out subsequent analysis, provide a kind of Gas-solid surface reaction unit and adopt it to carry out method for measuring.Gas-solid surface reaction unit of the present invention can carry out gas-solid reaction under high pressure, can obtain ultrahigh vacuum again; In high-pressure aerated and course of reaction, the online acquisition record of temperature, pressure can be realized, after gas-solid reaction, cavity can be made again to be in ultra-high vacuum state, again by other analytical equipment that sample vacuum transfer is extremely connected by sample Transfer pipe, thoroughly solve the problem that air pollutes material surface.Meanwhile, the present invention also provides the assay method based on this device, and the method can realize gas-solid reaction sample tests, and it is simple to operate, convenient to have, and measurement result is feature accurately, can meet the needs of Gas-solid surface reaction assay.The present invention thoroughly solves the secondary pollution of air to reaction surface, effectively improves work efficiency simultaneously.The present invention is reasonable in design, is skillfully constructed, and has great importance for Gas-solid surface repercussion study.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of Gas-solid surface reaction unit, comprise reaction chamber, the sample holder be connected with reaction chamber, pumped vacuum systems, aerating device, determinator, cavity is provided with in described reaction chamber, described cavity comprises high vacuum chamber, is arranged on the high-pressure chamber be connected above high vacuum chamber and with high vacuum chamber, the horizontal sectional area in described high vacuum chamber is greater than the horizontal sectional area of high-pressure chamber, and the top in high vacuum chamber forms the annular boss be connected with high-pressure chamber;
Described sample holder comprise be tightly connected with high vacuum chamber high pressure valve head, to be connected with high pressure valve head and high pressure valve head can be made along the elevating lever of high vacuum chamber relative movement, described high pressure valve head is also provided with the seal matched with annular boss;
Described pumped vacuum systems, determinator are connected with cavity respectively, and described aerating device is connected with high-pressure chamber.
Also comprise the form be arranged on cavity.
Described form is glass vision panel.
Described high pressure valve head is also provided with specimen holder.
Described seal is O-ring seal.
Described O-ring seal is fluorine cushion rubber or metal o-ring.
Described determinator comprise in pressure transducer, temperature sensor one or more.
Also comprise the information record carrier be connected with determinator.
Also comprise the sample Transfer pipe be connected with reaction chamber, the push-pull valve be connected with sample Transfer pipe, the pusher that is connected with reaction chamber.
Described pusher is magnetic force sample transmission rod or mechanical sample transmission rod.
Described pumped vacuum systems comprises molecular pump, mechanical pump, the vacuum tube that is connected with cavity, and described molecular pump, mechanical pump are connected with vacuum tube respectively; The gas-filled tube that described aerating device comprises high-pressure air source, is connected with high-pressure air source, described gas-filled tube is connected with high-pressure chamber, and described vacuum tube, gas-filled tube are respectively arranged with high pressure valve.
Also comprise the connecting pipe be connected with high-pressure chamber, described vacuum tube, gas-filled tube are connected with connecting pipe respectively, and described connecting pipe is provided with high pressure valve.
Adopt aforementioned means to carry out the method for Gas-solid surface reaction assay, comprise the steps:
(1) sample high pressure measures
Sample is placed on the high pressure valve head of sample holder, regulate elevating lever, make high pressure valve head rise to seal and annular boss close contact along high vacuum chamber, then in high-pressure chamber, be filled with required reacting gas by aerating device, by determinator record response situation;
(2) sample high vacuum obtains
Treat that step 1 is after completion of the reaction, regulate elevating lever, make high pressure valve head along high vacuum chamber decline, simultaneously by pumped vacuum systems by carrying out in cavity vacuumizing process, sample is in ultra-high vacuum environment.
Sample Transfer pipe is connected with analytical equipment, after being in ultra-high vacuum environment in cavity, opens push-pull valve, by pusher, sample is transferred to the miscellaneous equipment be connected with the present invention.
For foregoing problems, the invention provides a kind of Gas-solid surface reaction unit and adopt it to carry out method for measuring.When the present invention works, be placed in by sample on high pressure valve head, high pressure valve head can double as the effect of specimen holder, and by regulating elevating lever, make high pressure valve head rise to seal and annular boss close contact along high vacuum chamber, now, sample is in high-pressure chamber.Then, in high-pressure chamber, be filled with desired gas by aerating device, desired gas and example reaction, can be effectively measured sample by determinator, can temperature, pressure trend over time in online record high-pressure chamber.Adopt this structure, the volume of high-pressure chamber can be controlled in about 10mL, and in high-pressure aerated process, the vacuum tightness in high vacuum chamber can not be affected.After to be determined, regulate elevating lever, high pressure valve head is declined along high vacuum chamber, to carry out in cavity vacuumizing process by pumped vacuum systems simultaneously, sample is made to be in ultra-high vacuum environment, thus realize sample from low vacuum or positive pressure to the conversion of ultra-high vacuum environment, effectively avoid air to the pollution of material surface.
In the present invention, reaction chamber can adopt stainless steel to make, and component processing, inner surface treatment and assembling meet ultrahigh vacuum technological requirement.By coordinating of cavity and pumped vacuum systems (can being made up of mechanical pump and molecular pump), reaction chamber end vacuum can reach 5 × 10
-8pa.In the present invention, elevating lever (can adopt rotary spanner) can control the lifting of high pressure valve head, and high pressure valve head has been held concurrently the effect of specimen holder, also on high pressure valve head, can arrange specimen holder separately.
Further, also comprise the form be arranged on cavity, form can be glass vision panel; Mensuration person observes the change of sample surfaces state by glass vision panel.Seal is O-ring seal, and O-ring seal can be fluorine cushion rubber or metal o-ring, and user can select different sealing means according to different reaction systems.Determinator comprise in pressure transducer, temperature sensor one or more, also comprise the information record carrier be connected with determinator.
Further, the sample Transfer pipe be connected with reaction chamber, the push-pull valve be connected with sample Transfer pipe, the pusher that is connected with reaction chamber is also comprised.Pusher can be magnetic force sample transmission rod or mechanical sample transmission rod.By this structure, the connection of the present invention and other analytical equipments can be realized.Sample Transfer pipe being connected with needing the analytical equipment of carrying out measuring, after being in ultra-high vacuum environment in cavity, opening push-pull valve, by the pusher be connected with reaction chamber, sample being delivered to analytical equipment.Adopt which, both avoided the secondary pollution of atmospheric environment to reaction surface, and turn improved work efficiency.
Further, pumped vacuum systems comprises molecular pump, mechanical pump, the vacuum tube that is connected with cavity, and molecular pump, mechanical pump are connected with vacuum tube respectively; The gas-filled tube that aerating device comprises high-pressure air source, is connected with high-pressure air source, gas-filled tube is connected with high-pressure chamber, and vacuum tube, gas-filled tube are respectively arranged with high pressure valve.
Further, also comprise the connecting pipe be connected with high-pressure chamber, vacuum tube, gas-filled tube are connected with connecting pipe respectively, and connecting pipe is provided with high pressure valve.Adopt this structure, inflate and all realize by connecting pipe with vacuumizing, there is structure simple, the advantage such as easy to operate.
In the present invention, high-pressure chamber is positioned at above high vacuum chamber, and high vacuum chamber, high-pressure chamber form cavity jointly, simultaneously, high vacuum chamber, high-pressure chamber share a set of specimen holder, and this also makes the present invention carry out the gaseous tension coverage of Gas-solid surface reaction very extensively, can from ultrahigh vacuum to 2MPa.The present invention is reasonable in design, processing precise, in the process of high-pressure chamber inflation, the vacuum tightness in high vacuum chamber can not be affected, the volume of high-pressure chamber can be controlled in about 10mL, and this is very favourable to the consumption reducing rare noble gas or toxic and harmful.
In sum, the invention provides one and can carry out gas-solid reaction under high pressure, the reactive system of ultrahigh vacuum can be obtained again, the online acquisition record of temperature, pressure etc. in high-pressure aerated and course of reaction, can be realized; After completion of the reaction, cavity can be in ultra-high vacuum state, and by sample vacuum transfer to other analytical equipment be connected.The present invention had both avoided the secondary pollution of air to reaction surface, turn improved work efficiency, significant for Gas-solid surface repercussion study.
Accompanying drawing explanation
Fig. 1 is the cut-open view that the present invention does not form high-pressure sealed subspace.
Fig. 2 be the present invention form high-pressure sealed subspace analyse and observe constitutional diagram.
Fig. 3 is the structural representation of the embodiment of the present invention 1.
Mark in figure: 1, high vacuum chamber, 2, high-pressure chamber, 3, annular boss, 4, high pressure valve head, 5, elevating lever, 6, determinator.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
As shown in the figure, this Gas-solid surface reaction unit comprises reaction chamber, the sample holder be connected with reaction chamber, the form be arranged on cavity, pumped vacuum systems, aerating device, determinator, the sample Transfer pipe be connected with reaction chamber, the push-pull valve be connected with sample Transfer pipe, the pusher that is connected with reaction chamber.
Wherein, cavity is provided with in reaction chamber, cavity comprises high vacuum chamber, is arranged on the high-pressure chamber be connected above high vacuum chamber and with high vacuum chamber, and the horizontal sectional area in high vacuum chamber is greater than the horizontal sectional area of high-pressure chamber, and the top in high vacuum chamber forms the annular boss be connected with high-pressure chamber.
Sample holder comprise be tightly connected with high vacuum chamber high pressure valve head, to be connected with high pressure valve head and high pressure valve head can be made along the elevating lever of high vacuum chamber relative movement, high pressure valve head is also provided with the seal matched with annular boss.
Pumped vacuum systems, determinator are connected with cavity respectively, and aerating device is connected with high-pressure chamber.In the present embodiment, pumped vacuum systems comprises molecular pump, mechanical pump, the vacuum tube that is connected with cavity, and molecular pump, mechanical pump are connected with vacuum tube respectively; The gas-filled tube that aerating device comprises high-pressure air source, is connected with high-pressure air source, gas-filled tube is connected with high-pressure chamber, and vacuum tube, gas-filled tube are respectively arranged with high pressure valve.Further, also comprise the connecting pipe be connected with high-pressure chamber, vacuum tube, gas-filled tube are connected with connecting pipe respectively, and connecting pipe is provided with high pressure valve.
In the present embodiment, form can be glass vision panel, and O-ring seal can be fluorine cushion rubber or metal o-ring, determinator comprise in pressure transducer, temperature sensor one or more, pusher can be magnetic force sample transmission rod or mechanical sample transmission rod.Meanwhile, the present embodiment also comprises the information record carrier be connected with determinator.
During the work of this device, be placed in by sample on high pressure valve head, by regulating elevating lever, make high pressure valve head rise to seal and annular boss close contact along high vacuum chamber, now, sample is in high-pressure chamber.Then, in high-pressure chamber, be filled with desired gas by aerating device, desired gas and example reaction, can be effectively measured sample by determinator, can online record temperature, pressure trend over time.After to be determined, regulate elevating lever, high pressure valve head is declined along high vacuum chamber, will carry out in cavity vacuumizing process by pumped vacuum systems simultaneously, sample is in ultra-high vacuum environment, thus realizes sample from low vacuum or positive pressure to the conversion of ultra-high vacuum environment.Then, sample Transfer pipe being connected with needing the analytical equipment of carrying out measuring, after being in ultra-high vacuum environment in cavity, opening push-pull valve, by the pusher be connected with reaction chamber, sample being delivered to analytical equipment.
Embodiment 2 uses the present invention to measure active metal and high pressure H
2decomposition induction time
Experiment show active metal with high pressure H
2before kinetic reaction, have the induction period of certain hour, this, length was relevant to factors such as temperature, Hydrogen Vapor Pressure and hydrogen purities induction period.
Utilize device of the present invention can metal and high pressure H under Accurate Determining specified temp and pressure
2decomposition induction time.The affecting laws of correlation parameter to induction period also can be obtained by changing the experiment parameter such as temperature, pressure respectively.
Embodiment 3 uses the present invention to measure active metal and high pressure H
2reacted surface composition
Active metal and H
2reaction formed metal hydride in sample transfer process, very easily be oxidized by the oxygen-containing atmosphere in air, be difficult to by independent surface analysis equipment on-spot study surface composition.
Utilize device of the present invention, the surface after sample hydrogenation can not pollute by air.The H of active metal and specified pressure
2reaction terminates, unloading high pressure hydrogen after falling high pressure valve head, by sample transfer bar by sample vacuum transfer to the secondary ion mass spectrum (SIMS) be connected with the present invention or x-ray photoelectron power spectrum (XPS), study sample surface composition.
Embodiment 4 studies the CO/H of different pressures
2to the reducing action of metal surface high oxide
Utilize device of the present invention, by the CO/H of sample and different pressures
2after effect a period of time, unloading high pressure also, after falling high pressure valve head, rapidly by the x-ray photoelectron power spectrum (XPS) that sample vacuum transfer is extremely connected with the present invention, is studied oxide on surface variation of valence, is explored the CO/H of different pressures
2to the reduction effect of metal oxide.
Mensuration is used to show by reality, the present invention can realize in Gas-solid surface reaction, high-pressure aerated and the temperature of course of reaction, the online acquisition record of pressure, and after reaction under high pressure, sample can be made to be in ultra-high vacuum state, effectively prevent the secondary pollution of air for sample, meanwhile, sample can be transferred to rapidly in other analytical equipment be connected with native system carries out further research.The present invention not only thoroughly avoids the secondary pollution of air to reaction surface, effectively improves work efficiency again, has significant progressive meaning.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a Gas-solid surface reaction unit, it is characterized in that, comprise reaction chamber, the sample holder be connected with reaction chamber, pumped vacuum systems, aerating device, determinator, cavity is provided with in described reaction chamber, described cavity comprises high vacuum chamber, is arranged on the high-pressure chamber be connected above high vacuum chamber and with high vacuum chamber, the horizontal sectional area in described high vacuum chamber is greater than the horizontal sectional area of high-pressure chamber, and the top in high vacuum chamber forms the annular boss be connected with high-pressure chamber;
Described sample holder comprise be tightly connected with high vacuum chamber high pressure valve head, to be connected with high pressure valve head and high pressure valve head can be made along the elevating lever of high vacuum chamber relative movement, described high pressure valve head is also provided with the seal matched with annular boss;
Described pumped vacuum systems, determinator are connected with cavity respectively, and described aerating device is connected with high-pressure chamber.
2. Gas-solid surface reaction unit according to claim 1, is characterized in that, also comprise the form be arranged on cavity.
3. Gas-solid surface reaction unit according to claim 1, it is characterized in that, described seal is O-ring seal.
4. Gas-solid surface reaction unit according to any one of claim 1-3, is characterized in that, also comprises the information record carrier be connected with determinator.
5. Gas-solid surface reaction unit according to any one of claim 1-4, is characterized in that, also comprises the sample Transfer pipe be connected with reaction chamber, the push-pull valve be connected with sample Transfer pipe, the pusher that is connected with reaction chamber.
6. Gas-solid surface reaction unit according to claim 5, it is characterized in that, described pusher is magnetic force sample transmission rod or mechanical sample transmission rod.
7. Gas-solid surface reaction unit according to any one of claim 1-6, is characterized in that, described pumped vacuum systems comprises molecular pump, mechanical pump, the vacuum tube that is connected with cavity, and described molecular pump, mechanical pump are connected with vacuum tube respectively; The gas-filled tube that described aerating device comprises high-pressure air source, is connected with high-pressure air source, described gas-filled tube is connected with high-pressure chamber, and described vacuum tube, gas-filled tube are respectively arranged with high pressure valve.
8. Gas-solid surface reaction unit according to claim 7, it is characterized in that, also comprise the connecting pipe be connected with high-pressure chamber, described vacuum tube, gas-filled tube are connected with connecting pipe respectively, and described connecting pipe is provided with high pressure valve.
9. adopt device described in any one of claim 1-8 to carry out the method for Gas-solid surface reaction assay, it is characterized in that, comprise the steps:
(1) sample high pressure measures
Sample is placed on the high pressure valve head of sample holder, regulate elevating lever, make high pressure valve head rise to seal and annular boss close contact along high vacuum chamber, then in high-pressure chamber, be filled with required reacting gas by aerating device, by determinator record response situation;
(2) sample high vacuum obtains
Treat that step 1 is after completion of the reaction, regulate elevating lever, make high pressure valve head along high vacuum chamber decline, simultaneously by pumped vacuum systems by carrying out in cavity vacuumizing process, sample is in ultra-high vacuum environment.
10. method according to claim 9, is characterized in that, is connected by sample Transfer pipe with analytical equipment, after being in ultra-high vacuum environment in cavity, opens push-pull valve, by pusher, sample is transferred to the miscellaneous equipment be connected with the present invention.
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Cited By (3)
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| CN106814010A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院大连化学物理研究所 | One kind is based on surface of solids apparatus for measuring contact angle and measuring method under UHV condition |
| CN107024559A (en) * | 2017-02-24 | 2017-08-08 | 金华职业技术学院 | A kind of experimental method of use gas surface heterogeneous catalysis test device |
| CN109999726A (en) * | 2019-03-27 | 2019-07-12 | 华研环科(北京)科技有限公司 | High-temperature high-pressure in-situ XRD and XAS gas-solid reaction device |
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| CN109999726A (en) * | 2019-03-27 | 2019-07-12 | 华研环科(北京)科技有限公司 | High-temperature high-pressure in-situ XRD and XAS gas-solid reaction device |
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Application publication date: 20150506 |